Process of manufacture of an agglutinant for coatings.



' with an inert JEAN BOSEN, OI PABIS, FRANCE.

PROCESS OI MANUFACTURE OF AN AGGLUTINANT FOB COATINGS.

I Specification of Letters Patent. Patented July 30, 19l i.

No Drawing. Application filed July 30, 1914, Serial No. 854,161. Renewed Kay 29, 1918. Serial No. 287,367.

work, said coating or agglutinant consisting.

essentially of acid oils, heavy oils orwhat may be termed polymerized products of coal tar, petroleum tar (petroleum residues\ and the like. The products of this process being particularly characterized by the fact thatthe carbon or too hightly polymerized constituent that may have become insoluble in the products when raised to a temperature of approximately 80 C. is reduced to an extremely low percentage. To this end the process as carried on wit coal tars as the raw material will first be considered; in the first stage of the process, using coal tars, the latter are heated to drive ofl ammonia and other volatile products such as light hydro-carbon oils, these constituents of the raw material being removed by the usual method of distillation. After the ammonia and other volatile products.

have been thus eliminated the residue is subjected to a further distillation at a temperature ranging between 120 to 240 C., and which in any event must not exceed 250 C. In the accomplishment of this second distillation the residue is reduced to a la er of moderate thickness and, during disti lationg is constantly agitated by the'passage of acurrent of gas therethrough under a reduced pressure, some gas such as air diluted such as nitro n being used which at e temperature an prexure at which this second distillation occurs, is substantiall inactive in a chemical sense with regard to the substance through which it pases, the reason for this bei that it is highly desirable to avoid oxidation at this s'ta of-the pmeem.

distillates of this second distillation are then cooled and then condensed to re-.

move the solid product, naphthalene, crystallization and the remaining light 0 (hydro-carbon oils) may be subsequently re introduced into the residue.

1 The residue of the second distillation will a be found to mainly of the heavier hydro-carbon oils which are then oxidized or polymerized to attain the desired viscosity requisite of an agglutinant for the purpose set forth. The oxidization is carried on while the residue is in a comparatively thick layer and is effected by subjecting the same to the action of gaseous oxidizing agents such as air or oxygen which are allowed to bubble slowly'up through the residue under pressure, and while the residue is heated to a minimum temperature of say 250 C. The thickening of the residue is produced by the polymerization caused by the oxidizing agents and this is continued until the residue has reached a viscosity which substantially corresponds to 11 of Englers apparatus at 80 C. The resulting polymerized mass forms the product onsidering the treatment of petroleum tars or petroleum residue, substantially the same steps are carried on as in the case of the treatment ofcoal tarsabove set forth, that is to say the petroleum residues are first heated to remove the highly volatile oils; on having removed these constituents the residue is subjected to a further distillation at a temperature above 120 C. and not exceeding 370,C. This distillation is carried on while the residue is reduced to a la er of moderate thickness and, during the istillation, the residue is continuously agitated by the passage of a current of gas therethrough under a reduced pressure, some gas being used which, at the .tem erature and pressure at which the second d1stillation oecurs, is substantially inactive in a chemical sense with regard to the substancethroilgh which it passes, the reason for this being, as in the case of the coaltar process,that it is highly desirable to avoid oxidation at this stage of the process. 7 A sup lementary distillation of the residue is t en carried on at a temperature which may attain 370 C. as a maximum and the resulting product consist maml of I the heavy hydro-carbon )1lS which met en oxidized to produce the viscosity requisite of an agglutinant for the purpose set forth. This oxidization is carried on wh le the residue is in a comparatively thick layer and is efiected by subjecting the same to the acresidue while under premure, and while the residue is at a temperature-not in excess of 370 C. The thickening or increase in via,

cosity produced by the polymerization resulting from the action of the oxidizing agents is continued until the residue has reached a viscosity which substantiallycorresponds to 11 of Englers apparatus at 80 C. The resulting polymerizedmass is the agglutinant product formed by petroleum residues.

It will be. seen from the foregoing, that it is possible to produce an agglutinant by successively carrying on fractional distillation of either coal tar. or petroleum residues and then producing polymerization by the introduction of an oxidizing agent which results in the formation of agglutinants having new properties which are articularly desirable for the manufacture 0 those coatings used in iron work.

I claim 1. The process of manufacturing an agglutinant from hydrocarbon oils, which consists in heating the oils to distil off some of the light hydrocarbon oils and ammonia, then subjecting the mass being distilled to a further distillation at a higher temperature in the presence of an agitating current of gas or vapors to remove the naphthalene and other light oils, then reintroducing some 'then subjecting the mass being distilled to a further distillation at a higher temperature in the presence of an agitating current of gas or vapors to remove the naphthalene and other light oils, then reintroducing some of the distillate oils from the second distillate into the mass being distilled and redistilling and reintroducing until a heavv oil is obtained, and then polymerizing the re: sultant mass to the desired viscosity by causingv an oxidizing agent to bubble up through the mass. I

In testimony whereof I afiix my signature in presence of two witnesses.

JEAN ROSEN.

Witnesses:

ELY E. PALMER, J OHN BAKER. 

